CN104178350A - Method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum - Google Patents
Method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum Download PDFInfo
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- CN104178350A CN104178350A CN201410407139.8A CN201410407139A CN104178350A CN 104178350 A CN104178350 A CN 104178350A CN 201410407139 A CN201410407139 A CN 201410407139A CN 104178350 A CN104178350 A CN 104178350A
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Abstract
The invention discloses a method for separating and extracting chrysanthemum volatile oil, fiavonoid and phenolic acids from chrysanthemum. The method comprises the following steps: (1), crushing chrysanthemums dried in the shade, packaging the crushed chrysanthemums with filter paper, placing the packaged chrysanthemums into a soxhlet extractor, adding a low-boiling-pint organic solvent to carry out continuous refluxing and extracting until the color of the solvent is not increased, placing an extract into a rotary evaporator and volatilizing the organic solvent; then, adding distilled water and mixing, distilling in water, collecting the chrysanthemum volatile oil, after adding anhydrous sodium sulfate to dehydrate, and sealing and storing at a low temperature; (2), after volatilizing the organic solvent from the chrysanthemum residue, adding alcohol 8-12 times the amount of the residue to extract for 1-3 times, combining filtrates, recycling alcohol under reduced pressure, concentrating, freeze-drying, sealing and storing. According to a test, compared with a dual-extraction method, the method disclosed by the invention can be used for extracting the volatile oil which is remarkably more than the volatile oil distilled by virtue of the dual-extraction method as the chrysanthemum volatile oil partly contains active substances such as olein, borneol and camphor; and the extracting amount of fiavonoid and phenolic acids is nearly twice the amount of distillation raffinate.
Description
Technical field
The present invention relates to Chinese medicinal materials extractive technique field, relate in particular to a kind of method of minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum.
Background technology
Chrysanthemum morifolium has dispelling wind and heat pathogens, flat liver improving eyesight, clearing heat and detoxicating effect.Mainly contain volatile oil, flavonoid compound, phenolic acid compound.Pharmacological research shows, the main active substances of chrysanthemum dispelling wind and heat pathogens is volatile oils; The flat liver improving eyesight of chrysanthemum, anti-oxidant, the main active substances of repairing cardiovascular and cerebrovascular is flavonoid compound; Chrysanthemum is clearing heat and detoxicating, and anti-infectious main active substances is phenolic acid compound.
Chinese medicinal materials usually extracts after certain class material at present, and other a large amount of active substances are abandoned with the dregs of a decoction.Chrysanthemum is usually also to have extracted total flavones, has wasted volatile oil; Extract volatile oil, with the dregs of a decoction, abandoned flavonoid and phenolic acid etc.Also have kind of " a two formulation ", adopt distillating extracting oil, vinasse is as water extraction liquid.This method distillation time is long, temperature is high, and the volatile oil of distillation mostly is high boiling point; The extracted amount in the aqueous solution such as flavonoid and phenolic acids is few, and long-time high temperature extraction, also easily decomposes and destroy.
Summary of the invention
The invention provides a kind of method of minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum.
The present invention adopts following technical scheme:
The concrete steps of the method for minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum of the present invention are as follows:
(1) chrysanthemum powder drying in the shade is broken into 10-80 order powder, with filter paper parcel, put in apparatus,Soxhlet's, add low boiling point organic solvent to carry out continuous circumfluence extraction, carry to color in solvent and no longer increasing, by extract, put in Rotary Evaporators and fling to organic solvent, then adding distil water mixes, water distillation altogether, collect volatile oil of chrysanthemum, add after anhydrous sodium sulfate dehydration, cryogenic seal is preserved;
(2) the chrysanthemum dregs of a decoction are flung to after organic solvent, and add 8-12 and doubly measure, 50%-80% alcohol steep 1-3 time, merging filtrate, decompression recycling ethanol, concentrated, the airtight preservation of lyophilize, obtains Chrysan Yellow ketone, phenolic acids.
In step (1), preferably the chrysanthemum powder drying in the shade is broken into 40 order powder.
In step (1), described low boiling point organic solvent is ether and/or sherwood oil.
In step (1), the add-on of distilled water is 8-12 times of extract volume.
In step (2), preferably add 10 times of amounts, 70% alcohol steep 2 times.
In step (2), leach extraction method adopts: 60 ℃ of temperature of water-bath soak 1-3h, ultrasonic extraction 20-30min or one or more in 40-60min are extracted in thermal backflow.
Positively effect of the present invention is as follows:
The present invention first uses oil substances in organic solvent continuous circumfluence extraction chrysanthemum, and volatile oil is collected in water distillation altogether; 50%-80% alcohol steep Chrysan Yellow ketone and phenolic acid for the dregs of a decoction.This law can be extracted respectively separated compared with the volatile oil of chrysanthemum of top grade and Chrysan Yellow ketone and phenolic acid.Through repetition test, minute formulation of this invention compares with " two formulation ", and volatile oil of chrysanthemum partly contains by olein, borneol, camphor isoreactivity material, is significantly higher than the volatile oil of " two formulation " distillation; Because of flavonoid and phenolic acid, the solubleness in ethanol is greater than water, and after dregs of a decoction degreasing, chaff interference reduces, so flavonoid and phenolic acid extracted amount exceed nearly 1 times of vinasse.
Accompanying drawing explanation
Fig. 1 is extracting method flavonoid, the phenolic acid HPLC collection of illustrative plates of embodiment 3;
1. chlorogenic acid 2. galuteolins 3.3,5-O-dicaffeoylquinic acid 4.4,5-O-dicaffeoylquinic acid 5. Quercetins.
Fig. 2 is extracting method flavonoid, the phenolic acid HPLC collection of illustrative plates of comparative example;
1. chlorogenic acid 2. galuteolins 3.3,5-O-dicaffeoylquinic acid 4.4,5-O-dicaffeoylquinic acid 5. Quercetins.
Fig. 3 is the extracting method volatile oil GC-MS collection of illustrative plates of embodiment 3.
In figure, the material of number designation representative is in Table 4.
Fig. 4 is the extracting method volatile oil GC-MS collection of illustrative plates of comparative example.
In figure, the material of number designation representative is in Table 4.
Embodiment
The following examples are to describe in further detail of the present invention.
Embodiment 1
(1) chrysanthemum powder drying in the shade is broken into 10 order powder, with filter paper parcel, put in apparatus,Soxhlet's, add sherwood oil to carry out continuous circumfluence extraction, carry to color in solvent and no longer increasing, by extract, put in Rotary Evaporators and fling to organic solvent, then adding distil water mixes, water distillation altogether, collect volatile oil of chrysanthemum, add after anhydrous sodium sulfate dehydration, cryogenic seal is preserved;
(2) the chrysanthemum dregs of a decoction are flung to after organic solvent, add 8 times of amounts, 50% ethanol, and 60 ℃ of temperature of water-bath are soaked 3h, lixiviate 2 times, merging filtrate, decompression recycling ethanol, concentrated, the airtight preservation of lyophilize, obtains Chrysan Yellow ketone, phenolic acids.
In step (1), the add-on of distilled water is 8 times of extract volumes.
Embodiment 2
(1) chrysanthemum powder drying in the shade is broken into 80 order powder, with filter paper parcel, put in apparatus,Soxhlet's, add ether to carry out continuous circumfluence extraction, carry to color in solvent and no longer increasing, by extract, put in Rotary Evaporators and fling to organic solvent, then adding distil water mixes, water distillation altogether, collect volatile oil of chrysanthemum, add after anhydrous sodium sulfate dehydration, cryogenic seal is preserved;
(2) the chrysanthemum dregs of a decoction are flung to after organic solvent, add 12 times of amounts, 80% ethanol, and 40min is extracted in thermal backflow, lixiviate 3 times, merging filtrate, decompression recycling ethanol, concentrated, the airtight preservation of lyophilize, obtains Chrysan Yellow ketone, phenolic acids.
In step (1), the add-on of distilled water is 12 times of extract volumes.
Embodiment 3
(1) Flos Chrysanthemi of drying in the shade is ground into 40 order powder, take 100g and wrap up with filter paper, put in apparatus,Soxhlet's, add ether to carry out continuous circumfluence extraction, carry to color in solvent and no longer increasing, by extract, put in Rotary Evaporators 35 ℃ and fling to organic solvent, then adding distil water mixes, water distillation altogether, collect volatile oil of chrysanthemum, add after anhydrous sodium sulfate dehydration, cryogenic seal is preserved; (2) the chrysanthemum dregs of a decoction are flung to after organic solvent, add 10 times of amounts, 70% ethanol ultrasonic extraction 1 time, and 30min, decompression recycling ethanol, is concentrated into 200mL, the airtight preservation of lyophilize.
In step (1), the add-on of distilled water is 10 times of extract volumes.
(two formulations, two formulations are combinations of distillation method and water alcohol method to comparative example, can retain volatile component and the involatile constituent of medicine simultaneously.Zhang Zhaowang edits < < pharmacy of Chinese materia medica > > Beijing, China Traditional Chinese Medicine Publishing House, 2008 first versions, 252.)
Accurately take Flos Chrysanthemi meal 100g, put volatile oil extractor, add 1000mL distilled water, collecting volatile oil to volatile oil no longer increases (about 14h), and cooling 70min, reads scale, open tester lower end piston and remove the water of lower end, collect volatilization oil reservoir, use anhydrous sodium sulfate dehydration.Calculate the yield of volatile oil.Sealing is preserved.The vinasse filtering dregs of a decoction, after concentrating, add 70% ethanol precipitation 24 hours, get supernatant liquor, reclaim ethanol, and are concentrated into 200mL, sealing stored refrigerated.
Embodiment 3 (of the present invention minute formulation) is contrasted with comparative example (two formulation), and result is as follows:
Detect and result:
1, adopt ultraviolet-visible spectrophotometry to detect total flavones, total phenol
Two kinds of extracting method total flavoness of table 1, total phenol comparison
2, adopt HPLC method relatively Chrysan Yellow ketone, phenolic acids representative species
Two kinds of extracting method flavonoids of table 2, phenolic acid comparison
3, volatile oil yield comparison
The comparison of two kinds of extracting method volatile oil of table 3
4, volatile oil GC-MS comparison
Table 4 different methods extracts volatile oil component GC-MS and analyzes
Although illustrated and described embodiments of the invention, for the ordinary skill in the art, be appreciated that without departing from the principles and spirit of the present invention and can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited by claims and equivalent thereof.
Claims (6)
1. from chrysanthemum, minute put forward a method for volatile oil of chrysanthemum and flavonoid, phenolic acids, it is characterized in that: the concrete steps of described method are as follows:
(1) chrysanthemum powder drying in the shade is broken into 10-80 order powder, with filter paper parcel, put in apparatus,Soxhlet's, add low boiling point organic solvent to carry out continuous circumfluence extraction, carry to color in solvent and no longer increasing, by extract, put in Rotary Evaporators and fling to organic solvent, then adding distil water mixes, water distillation altogether, collect volatile oil of chrysanthemum, add after anhydrous sodium sulfate dehydration, cryogenic seal is preserved;
(2) the chrysanthemum dregs of a decoction are flung to after organic solvent, and add 8-12 and doubly measure, 50%-80% alcohol steep 1-3 time, merging filtrate, decompression recycling ethanol, concentrated, the airtight preservation of lyophilize, obtains Chrysan Yellow ketone, phenolic acids.
2. the method for minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum as claimed in claim 1, is characterized in that: in step (1), the chrysanthemum powder drying in the shade is broken into 40 order powder.
3. the method for minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum as claimed in claim 1, is characterized in that: in step (1), described low boiling point organic solvent is ether and/or sherwood oil.
4. the method for minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum as claimed in claim 1, is characterized in that: in step (1), the add-on of distilled water is that the 8-12 of extract volume doubly measures.
5. the method for minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum as claimed in claim 1, is characterized in that: in step (2), add 10 times of amounts, 70% alcohol steep 2 times.
6. the method for minute carrying volatile oil of chrysanthemum and flavonoid, phenolic acids from chrysanthemum as claimed in claim 1, it is characterized in that: in step (2), leach extraction method adopts: 60 ℃ of temperature of water-bath soak 1-3h, ultrasonic extraction 20-30min or one or more in 40-60min are extracted in thermal backflow.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513707A (en) * | 2014-12-16 | 2015-04-15 | 四川农业大学 | Method for extracting chrysanthemum essential oil and the extracted essential oil |
| CN107412292A (en) * | 2017-08-09 | 2017-12-01 | 长沙爱扬医药科技有限公司 | The method that general flavone and volatile oil are produced using malabar nut |
| CN111450131A (en) * | 2020-05-26 | 2020-07-28 | 四川馥芳集生物科技有限公司 | Method for simultaneously extracting volatile oil and chlorogenic acid from stems and leaves of ligusticum wallichii |
| CN112057369A (en) * | 2020-10-15 | 2020-12-11 | 天津科技大学 | Preparation method and application of golden-silk-Huang chrysanthemum volatile oil with whitening and freckle removing effects |
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| CN103952240A (en) * | 2014-05-19 | 2014-07-30 | 安徽科技学院 | Preparation method of abelmoschus manihot essential oil |
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| CN103952240A (en) * | 2014-05-19 | 2014-07-30 | 安徽科技学院 | Preparation method of abelmoschus manihot essential oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104513707A (en) * | 2014-12-16 | 2015-04-15 | 四川农业大学 | Method for extracting chrysanthemum essential oil and the extracted essential oil |
| CN104513707B (en) * | 2014-12-16 | 2017-07-28 | 四川农业大学 | A kind of extracting method of chrysanthemum essential oil and the essential oil of extraction |
| CN107412292A (en) * | 2017-08-09 | 2017-12-01 | 长沙爱扬医药科技有限公司 | The method that general flavone and volatile oil are produced using malabar nut |
| CN111450131A (en) * | 2020-05-26 | 2020-07-28 | 四川馥芳集生物科技有限公司 | Method for simultaneously extracting volatile oil and chlorogenic acid from stems and leaves of ligusticum wallichii |
| CN112057369A (en) * | 2020-10-15 | 2020-12-11 | 天津科技大学 | Preparation method and application of golden-silk-Huang chrysanthemum volatile oil with whitening and freckle removing effects |
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Application publication date: 20141203 |